Removal of granular solids from liquid-solids contacting systems



5 sheets-sheet 1 E. R. KENT ETAL CONTACTING SYSTEMS REMOVAL OF lGRANULJR SOLIDS FROM LIQUID-SOLIDS Feb. 1s, 1960 Filedy Oct. 17, 1956 I A /3 a4 INVENToRs v ATTORNEY fn'f` E Emi mriy Z. Payne fa/m Mls'e BY ffm Feb. 16, 1960 E. R. KENT ETAL 2,925,382

REMOVAL oF GRANUL'AR soLIDs FROM LIQUID-somos CONTACTING SYSTEMS 5 Sheets-Sheet 2 Filed Oct. 17, 1956 rtm'yf. 4W

//Zse INVENTORS Feb. 16, 1960 E R KENT 5m l 2,925,382

REMOVAL 0F GRANLA'R SOLIDS FROM LIQUID-SOLIDS CONTACTING SYSTEMS Filed Oct. 17, 1956 5 Sheets-Sheet 3 -hmq Amm

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.ff/iwf /Zs'g yINVENTORS ATTORNEY Feb. 16, 1960 E. R. KENT ETAL 2,925,382 v REMOVAL OF GRANULAR SOLIDS FROM LIQUID-SOLIDS CONTACTING SYSTEMS Filed Oct. 1'7, 1956 5 Sheets$heet 4 Olz PRESSURE mop /fv .5E/1L cazaMN-Pm//vs PH? .sam/ff /A/f/ Pm mar o1o A 0.2 0.4 0.6 0.8 1.0 1,2

INVENTORS R KENT ETAL 2,925,382A

` E. REMOVAL OF GRANULAR SOLIDS FROM LIQUID-SOLIDS CONTACTING SYSTEMS Filed 061'.. 17, 1956 5 Sheets-Sheet 5 Feb. 16, 1960 v S ginas w50] a 0.5 'T 0.4 um 0.3 :k a..

0.1 L0 2 1o 1z 14 Eric i?. Pien/Z Fundy Z. Payne fhnf Wise INVENTORS Am ATTORNEY V Continuous Percolation process. Adsorbent such as fullers earth, bauxite, etc., is gravitated from a flow splitting device through passages. 11 into treater 12. The adsorbent 'gravitates through treater 12 as a columnar mass, that is, a mass in which particles move substantially unidirectionally downwardly as opposed to a uidized mass Ywhere the' particles move about in rann dom motion. ln theV columnar mass the particles may or may not Vrest upon each other at all times. Liquid oil is supplied'through passage t3 to the lower section of this columnar mass. This oil may be at any desired temperature but is usually heated, for example, to about 300 -F. The oil ows upwardly through the mass to undergo the desired treatment which may be, for eX- ample, decolorization, filtration or fractionation. The treated oil is removed through passage 14.

trated in Figure 3.

veyor 35 discharges solids intoconduit 36 from which they pass into the upper section of flow splitting device l The process and apparatus of this invention, by means of which uniform solidswithdrawal is achieved, is illus Within the lower ,section of passage i2 ismaintained a plenum space 37 which is filled with the liquid charge material supplied thereto through passage 13. This liquid charge passes from plenum space 37 into the lower end of the oolumnar'mass 387through a plurality of spacedinjection nozzles 3 9. These nozzles may be of a variety of constructions but preferably are of the type described and claimed in United States Used adsorbent gravitates from treater 12`downwardly Y i" through a plurality of passages 15 as a plurality of seal columns by a mechanism which is explained in greater detail hereinbelow. The adsorbent is suspended in liquid oil within the lower section of passages l5 and passes as a uidized stream to withdrawal passages 16. The streams flowing through passages 16 are redirected so as to flow downwardly and are then combined proportionately in a conical combining chamber 17. From the lower end of chamber 17 adsorbent and oil, still'existing with the adsorbent suspended in the oil, are removed. through passage 1S and ow upwardly throughthat passage. The suspension is removed through one of outlet passages 19. The rate of removal is controlled by selective choices among passages 19 in the manner taught in United States Patent 2,783,189 to Bergstrom et al. All

ofpassages 19 lie beneath the liquid level 2@ maintained in treater 12. The difference in hydrostatic head oetween the one of passages lli? used as an outlet and liquid level 20 acts to force the adsorbent through the withdrawall system.V Therefore,'the rate of adsorbent flow from treater 12 may be adjusted by selective choice among outlets i9. A higher outlet will give a lower ow and a lower outlet a greater ow. The solidssuspended in oil pass out ofrpassagel9 into Vconduit 2liV Vandfall downwardly therethrough into the `upper end of alwasher 22. v

Within washer 22 liquid oili which enters with the adsorbent is dissolved in a suitable solvent. The adsorbent flows through the washer normally as a compact column.

The solvents which may be used include carbon tetra.

Chloride, normal heptane, octane and the like, and petroleum naphtha. A preferred solvent is a paranic naphtha boiling within therange Mtl-300 F.

Solvent is supplied through passage 23 and the sol-V vent-oil solution removed through passage 247i. Typically, solvent will be supplied at a temperature within the range 60-250" F. Adsorbent gravitates from the lower Patent 2,772,780v to Penick. From the lower end of columnar mass 38, adsorbent gravitates downwardly through conduits 15 as a plurality of conned, substantially compact seal columns 40. Together with the adsorbent in4 columns 40 a quantity of liquid oil also passes downwardly through passages 15. Conduits 16 are equipped at their upper ends with inverted U-tubes of goosenecks di, the downwardly facing open inlet ends of which are situated within the lower section of columns liti. The liquidoil which ows downwardly through colhi pended'as the entire withdrawal stream is redirected into a downward direction in the main portions of conduits 3.6. These suspensions are then combined within a combining means like funnel t7.

The process and apparatus of vthis invention clearly i" have certain advantages overthe priorart. The multiple liquid-solids lstreams are combined-while the solids are separated byvliquid (liquid in continuous phase)` rather than while the Ysolids are in compacted condition (solids in continuous phase); Clearly, a more u niforrnc'ornbination can be obtainedwhen the streamsV have the fliquid in the'- continuous 'phase lrather than fthesolids Abecause of the greater ease with ywhich'the Vsolids will{me'r`ge"in this flow condition'as opposed to that where the indi- V, vidual solids 'aie so close to each other that they touch.V

. .65 bed within the drier, uidization being effected by a gas"v such' as a vaporized portion of the solvent naphtha or.

steam supplied to conduit 3?.V Heat may alsov be sup-L ,Y

plied to the bedby means of a heat transferrmediurn supplied through passage 31 and removed through passage 32. Fluidizing gas and vaporized solventrnay be removedrthrough conduit 33 anddried adsorbent passes from drier 29 through conduit 34 intol the lower end of a conveyorSS. This conveyor maybe of any desired construction such as a bucket elevator or a gas lift. Con- A further advantage of thisY vinvention is that it atall times` maintains seal columns 40 vin compact condition.

lThis isimportant since these columns act as the primary control to avoid large quantities of solids from being removed frorn themass above by the'owing liquid. With prior artsystemswh'erein itfwas attempted to'use valves for control on the compact sealcolumns or on a cornpact stream into which the columns had been combined,

or wherein a lift oil was added to the combined suspension to elevate it, very often someof theV seal columns would'assume the type.V of flow-in whichtheVVV liquid isfinA the continuous phase.v Thesecolumns would, therefore,

flow substantially faster than the remainder of the co1- umns. This would cause differencesin `owA rateacross the massvin the contacter and resultant lno n-uniforn'l'contacting. If a sufficient numberV of Vthese columnsV assumedA this type of ow, the greatly'increa'sed raterof withdrawal" `ow there willbecarriedbyhe liquid to the upperV end ofthe seal column the sari-ie.quantity'of'solidslas` are removed from thelower" end and it will Vat all times Yremain compact". v' *i Y A further advantage of this invention is that it is self-A starting. When there is a shutdown of the unit in which it isfemployed, adsorbent will', collect compacted condi#v tion at various pointsV in thewithdrawal system, forex:y

ample, in the transport passage, When the unit is then seopefof tonormloperation.; Y- i i i V.'Ifhlelevaref'oertairl requirements necessary 4.to ,the voperation fsatgiven.systemeaccordingrgto.thisfinvention The seal column:40mustealways-belargerthan1the withdrawal Y ypassage 16 and .gooseneckf411z .The minimum ratio i areas 'of :these itwo :u'1ill"va1'y, @depending upon y thesize range sof :.-solids employed, ithewiscositylof the #l lduidglrlensity of;the1;solids,.-andithe pressure-drop main# .i y

tainedr'zacrossztheisealfolumn. lThis ,ratiov cannot tlr fore, be sety forth'with'exactitude vfors'eachwand sys-` tem 'tin VVwhichnthisv inventionmightfbe employed. .-Ho ever, there is :shown in Figure@ :the minimum: ratioof .pipe Lof :':iucreasing size .could :tbe :.used with Ywithdrawal streamscentering :at-@different:vertical-points.` 'With y.col `lector i177 zitfis: preferred that there bezrmaintained :a conical combined awhile" iloving'V :downwardly y ilorfiexainple, 'ra

roof 45zthereinzso that'thescombiningoccursf*insan-aannular `downwardly tapered/stream. yWhenfusingJcollectorf :CitY

Y is preferable that'pipes 16 enter its upper end .inazrn'g i toremovesolidsirom.theasealcolumnsandreturnthe unitH f tiplefgoutlets, illustrated in.Figure2,.need notbe used zto l5'V kshaped pattern. DetailsDfasatisfactorycollector of this type will -ibe found in UnitedV States patent application l The tlowl controldevlice of UnitedStates .patent:appli-- cation ISerialNumber1424.956.,l filed rApril 22, .11954,involvingan upwardlyrdirected:transportpassage-withxmuh Opening.;dviegsuchaskavalye inpassage 18,;to effect flowqc'ontldl. providedtheisolidsaresuiciently :separated by-liquid thatitheywill not, uponthrottling, grevert'vtoithe Y flowy condition'whereinz-.the solids are lin the continuous seat-column -area to withdrawal passagesarea .at the inlet i to `.the withdrawal ipassage thatmustxbe maintained .zwith Y a variety of pressure drops across fthe seal .columns,f1dif ferent types .of adsorbents and.aclsobentzsize.rar1ges,.and oils with :differentwiscosities For each of these isystems to operate -accordingtothis invention theratioiofthe seal column area to .withdrawal Ypassage inlet area :shouldn .be above. this .minimum ratio. :In :Figure4f each of l-the glin'es bears the name-.ofthei-adsorbentgto whicliiit relatesffeg., bauxite. The numerals before the' 1adsorbent,narriediifn` dicate-:the size rangeoftheradsorbentvtowhichlthe .curve applies.- Forfexample, 60,;indicat'esrtl1'at theeadsorbent A3.352grarris per cubic centimeterjwhile-the120/6Oimesh bauxite had a true densityof 3.404 grams per `:ubicic:entiv meter. LVData similar -tolFfigure 2l Y'can be routinelyjde'- phaseandthuscause the flow controldiculties noted in i capacity. as', great :as and preferably greaterv thani transport f-particleswere of sizes :distributed betweenLZOjra'rid 6r01mesl1" Y Tyler. Thefnumerals Aafter-theadsorbent named, terg.,

connection'.with%the:ldiscussion of Figure 1* tooccur.

When the` `sojlids'l-ate control :system illustrated lis fem-v passage-18, so tha'tfthey impose no fow restriction on the suspension Vllowug from the transport pass'age. VWithin the transportjpassagel-the lveloeity should be atlleast 0::1.

seooneLfan preferabl -per.s`econd.;

'lio ld'notgbe v.greater than 4fffeet I method and-@apparatus ofi-this :invntionwas .'tefsted'"V 1n a'pilotplant in.which 3;seal'legfconduits, each 'made' off/.4-1nch';pipaextended;downwardly from an' enclosed inch pipe-.as was :.thefj; transport passage. .The :data of velopedjfor any other system. ""It rca'nbesaid thatgener-l ally, for vmoist systemsjthe ratio ofsel column area '1towithdrawal passage inlet area should be greater thanlOl and preferably greaterthan 25. Y Y

"It is falso-a -requirement of this inventionth'at the -su'spensions ov'ving .in the withdrawal passages' be'corribirie'dv while flowing downwardly and-notupwardly'. Tests 'have y shown that upwardly flowing suspensions do-not combine uniformly `and proportionately. i Y Y .y

V'As explained in United States patent application'Serial Number 237,267, filed July 117', 19511, the jseal columns'40 sl'lou'ldbeV spaced across the lower end of columnar-mass 38-so as tojeffectproportionate withdrawal-therefrom In order that all of the'solids'iriV mass 38 will be readily accessible to--a seal column and ,"deadfspacesY in the mass Y Willbe'avoided, each `seal;columrrshould-serveless than 1'7 square vfeet and preferablylesssthan, 1'2 square'y feetof columnar mass 38. lThese seal columns are restrictiedfarea compared lto tlie'm'as's-and -ingeneral their totalcross#v 'A sectional areashouldbe less 'than' IOpercent o'ffthetbtll horizontal"cross-sectional? area' off ma'ssBSf' ,'Seal columns;

equal{cross-sectional.'v area. arid,v `thereforer,`1 uniformly dis- A tributed-:with .frespectttoarea-across the lower-feudo mass i 3&5 rHowe-Yn;itfisiwithinzthe,broader-lscopeoimi iu- Y uentionthatzthey.befoffdiffcringfare with' propriate'tosuhareas. E

Aefr-fthegtype-U ingested f,

vEigure 5a show that the flow iratel was :completely control-y lable.- The quantity fpressure drop :in-.- seal fcolumn` vwas' used vbecause-'it isa :measure ofthe driving''force operating to regulate theadsorbentrate; L y

Figure 6j demonstrates,that'thefsolids ow; rate will maintainitself constant vusing `this :invention indefinitely. The s lightl'variations inrateshown inaFigure 6 are -within theexpe'rimental accuracy of thedeterminationsthereof- Figure A7 illustrates the effect ofthe/viscosity of thevoil on flow' rate inl this experimental unit. c

All ofthe data in Figures '5L-71wer'etaken `on a system employingl 11S-30 mesh Tyler .fullers nearth. V,An oil of Sarcentipo'ises viscosity -at 70-"..F. was usedtoobtain the' dataofFigures 5` and 6. Y

-This invention should be understood to cover all changes and modifications of the examples of the 'invention herein chosen forfpurposes ofdisclosure which do not constitute departures from thespiritand scope` of the .invention.

Vfl A method forjthe'controlled withdrawal ofy granular solids from a confinedlliquid-solids,contacting zone, which comprises: removingl Vgranular solids fromjthe contact- I. ing zone asta plurality o f confined;"substantially/compact Vs.ealefcolumris throughj-whichf'liquid 'fromthecontacting Y zone ows; passingsolidsaud liquid `from each Iof said seal columns into a `separate-jconfined withdrawal 'passage 'havmga downwardly? facing 'open inlet-.irl free communi;

- l cation` I,witlfr-fsaid rseal ,column :maintaining each Withdrfawaleparssage. sucientlyj. smaller'fthan th'e: sealc`olmn: withzwliich.itgommunicates that .theliquid-.zentezsflthe withdrawallpassagefrom the s'eal colurrnzfat afvelocity suficient'sto lift ,solids-:.fromftheYlowerfend of'lth'e seal,y

column into j fthe :Withdrawal #passage andlrinaintain the tainingjilhe suspension Vofgi solids v inf each said 'suspension while confined to lio'w'na down-` wardly direction; combining all of thesuspensons fromv all of the withdrawal passages while said suspensions are flowing downwardly andrforming therefrom a single combined suspension; regulating the flowrof solids from said contacting zone by regulating the ow of said combined suspension. f

2. A method for the controlled withdrawal of granular solids from a confined liquid-solids contacting zone, which comprises: removing granular solids from the contacting zone as a plurality of "conned, substantially compact seal columns whose total cross-sectional area is less than the cross-sectional area of 'the' contacting zone and through which liquid-from the contacting zone vows; maintaining a separate confined withdrawal passage in' free vand open communication with the lower section of each of said sealf columnsfthroug'ha downwardly facing open inlet;v maintaining each withdrawal 'passage' suiciently smaller thanthe seal column with which it com- Y the withdrawal passageit is accelerated in velocity and lifts solids from'the lower end of the seal column into the withdrawal passage and maintains the solids suspended inthe liquid as it iiows upwardly into said passage; after entrance of the suspension into the withdrawal passage redirecting its flow to a downwardly direction; combining all of the suspensions from all of said withdrawal passages while said suspensions are ilowing downwardly and forming therefrom a single combining suspension; passing said combined lsuspension into and through a transportrpassage and'adjusting therate of ow of solids from said contacting zone by adjusting the level ofdischarge from said transport passagev relative tothe liquid level in the contacting zone.A

3. The method of claim 2v further limited to: a contacting zone in which'the solidsexist as a columnar mass; the'ratio Aof the area of the seal column to the area of the withdrawal passage being greater than 10; the' transport passage extending upwardly and having a plurality of discharge'passages connected thereto at a plu-` rality of spaced vertical levels, all of which lie below the liquid level in theY contacting zone and all of which are of sucient size so as not impose a tlow restriction on the iiowing combinedv suspension; and controlling the rate of solids removal from the solids contacting zone by selectively withdrawing the combined `suspension throughthe one of said discharge passages suitable to give the desired flow while permitting no withdrawal through the other'discharge passages, an increase in flow* being Aaccomplished by using a lower discharge vpassage and thereby lowering the level of withdrawal from a transport passage, while a decrease is effectedV by using a higher discharge passage and thereby raising the level of withdrawal from the transport passage.V

4. In a process for the decolorization of liquid hydrocarbons by owing the liquid hydrocarbons upwardly through a downwardly moving columnar mass of granular adsorbent, a method for withdrawing the adsorbent uniformly from the lower section of the columnar mass, which comprises: withdrawing a plurality of conned, substantially compact streams of adsorbent mixed with some liquid hydrocarbons from a plurality of points uniformly-.spaced and distributed across the lower section of acolumnar mass at a common level, the total crosssectional area of said streams being less than the crossV` sectionalarea of said columnar mass at the level of with-v drawal; maintaining,V any upwardly extending withdrawal passage in open communication'with the lower end of each of: said'streams through a downwardly facingy open inlet; maintaining each withdrawal passage sufficiently smaller'than the stream with whichit connects that" the liquidwhich isY flowing through said .stream'acceler'ates asit enters said withdrawal passage sutlici'entto =lift the Y pension.

solids from the'streaminto thewithdrawal passage and: maintain the solids suspended in the liquid as it tiowsl upwardly into the passage; directing each of said su's-` pensions downwardly after entrance'into the withdrawal passage and combining all of said suspensions uniformlyy and proportionately while they are flowing downwardly' into a single combined suspension; flowing said combinedv suspension upwardlyinto and through a transport passage and withdrawing the combined suspension from the transport `passage through-one of Va plurality of outlets maintained below the level of liquid in the contacting zone; regulating the yrate atewhch adsorbent ismoving from the contacting zone by selective choice amongzthe plurality of outlets, a'higher'outlet being used to .reduce the ow rate and a lowerone to increase it. Y t

5.InV a process Afor the countercurrent contactingof liquid'hydrocarbons and granular adsorbentsl wherein the liquid hydrocarbons are passed upwardly through'a down' wardly moving columnar mass of adsorbentmaintained within a confined percolation-zone, 'a method'for with-A drawing adsorbent from the lower end of the columnar;

mass so as to effect uniform movement of a columnar `mass, which comprises: withdrawing adsorbent particles together withv some of the liquid hydrocarbons from a plu-v4 rality of points uniformly distributed acrossv the lower section of said columnar mass as a plurality of conned,sub stantiallyY compactV streams of adsorbent particles, the to tal cross-setcional'area of said streams being less than the stream with which itV communicates so that the liquid enter the withdrawal passage from the stream ata velocity suflicient to lift adsorbent. particles from the lower end of the stream into the passage and maintain the particles suspended in the liquid as it ows'upwardly into the passage; restricting the suspension within the withdrawal passage to a downwardly flowing direction and combining-all of said suspension from alllof said withdrawal passages into a single confined combined suspension and regulating the rate of adsorbent withdrawal from the percolation zone by regulating the rate of ow of said combined sus- 6. The process of claim 5 in which the ratio of the cross-sectional area of each of said streams to the crossf sectional area of the withdrawal passage'with which it communicates is greater than 25. y

7. `An apparatus for the continuous countercurrent contacting of liquids and granular solids, which comprises in combination: an enclosed contacting vessel; means for supplying granularrsolids to the upper section of said vessel; means for supplying liquid to the lower sectionof said vessel; means for removing liquid from the upper section of `said vessel; a plurality of solids withdrawal conduitsconnecting into the lower end of said .vessel and extending downwardly from aV plurality otV horizontally spaced points uniformly distributed over the crosssectional area of said vessel, said conduits being equal in size and sulicient in number so that there is less than l2 squareA feet of vessel Vhorizontal cross-sectional area for eachfwithdrawal conduit; a return-bend associated with each of said `withdrawal conduits, the ratio'of Athe crosssectional4 area of the conduit tojthe cross-sectional area`v of the; returnzbend being greater than 10, one downwardly facing open end of each returnbend being located within said conduit and-'the other extending downwardlyto a level therebelow; an upright symmetrical funnel Vmember situated beneath VVsaid contacter, ythe'erid's 'of' allV of saidfretumbends connecting into'the upper end vof said funnel imemb'er; f members VVdefining va transport passage way lextending from the lower end of said-fur'mel"in'etberI upwardly and members defining a plurality of outlet pasl 9 sageways and means for selectively opening and elosing said outlet passageways.

References Cited in the le of this patent UNITED STATES PATENTS 5 2,631,727 Cichelli n ...1--- Maf. 17, 1953 10 K Berg n July 27, 1954 Daniel Oct. 5, 1954y Kollgaard Feb.`1,k 1955 Mertes et al May 15, 1956 Bergstrom et al. Feb. 26, 1957 l Attesting Ofcer UNITED STATES PATENT OFFICE CERTIFICATE 0F CORRECTIN Patent No. 2,925,382 February 16, 1960 Elric R. Kent et al.

It is herebjf certified that error appears in theprinted specification of the above numbered patent requiring correction and that the said Letters Patent should read as corrected below.

` Column l,l line 29, for "understod" read understood line 4l! for "variatn" read Variation wg column 3, lin 32, for "choces read choice column 4, line 25, for v "soil" read solid -y column '7, line 43Xt for "not impose read not to impose column 8,T line 28 for "crosssetconal" read cross-sectional Signed and sealed this 27th day of September 1960..

' (SEAL) Attest:

KARL H0V AXLINE ROBERT C. WATSON Commissione;` of Patents 

